Process for the distillation of alcoholic liquids.



E. GUILLAUME.

PROCESS FOR THE DISTILLATION 0F ALCOHOLIC LIQUIDS.

APPLICATION FILED MAR. 26, 1902.

996 ,328, Patented June 27, 1911.

WTNESS as:

INVENTOR,

unrrnn STATES i g rnntr OFFICE.

EMILE GUILLAUME, OF PAIR-IS, FRANCE.

PROCESS FOR THE DI STILLATION OF ALCOHOLIC LIQUIDS.

Specification of Letters Patent. Patented June 27, 1911.

Application filed March as, 1902. Serial no. 100,033.

the so-called head and tail? products.

By head products are meant those impurities having a lower boiling pointthan ethyl alcohol; by tail products, those whose boiling point ishigher than thatof ethyl alcohol. Under head products may be includedthe aldehydes, ethers, and the like, while tail products embrace suchimpurities as amyl alcohol, isoalnyl acetate, isovalerate of ethyl, etc.1

My process is based. upon the fact that when a liquid alcoholic mixturecontaining ethyl alcohol and impurities having'a higher boiling pointthan ethyl alcohol is suflicientlv diluted with water, the eth 1 alcoholmay be separated by distilling 0 said impurities and be recoveredpractically pure, diluted only with water. For example, take a mixturewhich contains ethyl alcohol (boiling point 78 0.), and amyl alcohol(boiling point 132 C.) and'dilutewith water until mixture marks 137 onthe Baum hydrometer. lrVhen this point is reached the amyl alcohol willbe vaporized 2.5 times more rapidly than the ethyl alcohol and the ratio40 of amyl alcohol to ethyl alcohol in the distillation vapors will be2.5 times that in the liquid mixture. In other ords, the addition of theproper amoun of water has caused the ethyl alcohol to act like a tailproduct as regards the amyl alcohol.

With my present process I have found in practice, that when treatingcrude distillates, in order to obtain a complete separation of the ethylalcohol constituent, the liquids should be diluted with water until theymark 13.7 to 14.3 Baum, and should be main- 7 tained at this degree ofdilution.

In the annexed drawings I have shown, as an example, an apparatus for.carrying out my process, which on a proper scale will be sufficlent toallow a production of 6500 pipe 0.

liters calculated as absolute alcohol daily. Qf course, the size anddetails would be varied to meet local conditions and requirements, butthis apparatus will carry out my process perfectly.

In the drawings 1, 2 and 3 indicate superposed communicating distillingcolumns, rovided wit-h shelves consisting of perorated plates p having asuitable overflow In the illustration chosen the column 1 has a heightof approximately 2.5 meters, :1 diameter of 800 mm., and contains 14plates; column 2 is 1.8 meters high, 750 mm. in diameter and has 11plates; column 3 has 11 plates, is 1.8 meters high, and its diameter 1s650 mm. At the base of column lsteam enters, in the direction of thearrow 8, into the coil 37 31 is the outlet, controlled by cock 32.

Arrows 1,, l 1, indicate direction of flow of liquids into and in column1, e the direction of liquids in column 2, and t,, t,, flow of liquidsin and out of column 3. The direction of vapors in the columns is markedby arrows 0,, 1),, h h while it, indicates the flows of the condensedhead products. At the top of column 1 is the inlet pipe 4, controlled bythe cock 6, and into the top of column 2 enters the pipe 5, providedwith cock 7, w indicating the direction of flow. Above column 2 iscolumn 3, opening through 23 into the condenser G, which in turn,through pipe 28, is connected with the refrigerator R, provided withpipes 41 fastened to bases 42. The condenser G is built up of pipes 38fastened between bases 39, and supported by perforated plates 40.

24 is a closed pipe against which the vapors coming through the passage23 impinge and are distributed among the coolingpipes 38.

14 is a cleaning plug hole, and 44 the outlet of condenser O.

43 is the inlet for water to refrigerator R.

25 is a vent-pipe and 21 a return pipe from the base of It, in thedirection of c, to a point above the base of condenser C.

22 is a pipe connecting the base of R with the sampling tube 12. Adischarge pipe 9, furnished with a plurality of tap-cocks 8,

vconnects the base of column 3 with the refrigerator 10 and the samplingtube 11. The The condensing water enters at 43 and leaves therefrigerator through, the pipe .29, passing to the condenser C, the flowbeing indicated by the arrows e0 'w w and 10,. For

automatically controlling the flow of water with the condenserv and anoverflow pipe .hole, interposed in one of the 20 emptying ,into the topof column 3, is joined to the float box 16 byJa pipe 35. A diaphragm,perforated with a very small ipe connections 36 retards sufficiently theow between the vessels 15 and 16 and avoids shocks. Should the pressurechange in the condenser chamber C, such variation is transmitted throughpipe 19, container 15, pipe 35', float 18 to valve 17 and the watersupply is thus regulated.

The operation of theprocess is as follows: The apparatus is first heatedand main-' tained heated by the steam pipe 30 at a temperature (circa96-97 C.) sufficient to separate the alcohol from the liquid that thetop of column 2, through the pipe 5.. This dilutes the ascending vapors,and is enters the column 1. The liquid to be treated, consistin of ethylalcohol, head products and tall products, having been previously dilutedto mark 13.7 to 1.4.3 Baum, is introduced by the column 1. The liquithus introduced has a temperature of approximately 60 0. While thediluted liquid is flowing down over the plates of column 1, the headproducts, the tail products and some of the ethyl alcohol are vaporizedand pass upward into column 2, while the unvaporized diluted ethylalcohol falls-tothe bottom of column 1, and is drawn off through pipe31, provided with valve 32. The ascending head products, tail products,and the ethyl alcohol therewith entrained are met, as they ascend incolumn 2, b a mass of hot water, low wines or s milar 1qu-1d, mtroducedinto added in sutficient amount to maintain the dilution, in column 2 1at 133 to 14.-7

-Baum, the specific gravity atwhich the head and tail products willdistil off from What ethyl alcohol there may be still carried along incolumn 2 by the head and'tail products. As the amount of dilution isdependent upon the temperature, and in order to enable the operator tomaintain an approximately unifoym dilution in column 2,

thermometers 33 and 34 (of any construe-- tion) are provided at thebottom and at the top of column 2, and during the operation the readingsof these thermometers must be kept approximately equal. When thesethermometers read 96 to 97 0., the operator knows that the density ofthe liquids is at 13.7 to 14.3 Baum and that the ethyl alcohol will actin relation to the head and tail products in the vapors, as a tailproduct. The vapors rising in columns 1 and 2,

pipe 4 into the top of' meet the entering water. The ethyl alcohol. hasgreat affinity for it, and being readily soluble therein unites with thewater and finally reaches the bottomof column 1,.while the tailproducts'being insoluble in water ass through it and upward into column3. [be head products are soluble iii water, but

their boihng'points bein so much lower than the water vapor,'an their var tension being so much greater,the a ass through the water with thetail pr nets. and up into column 3. In column 3. the vapors consist oftail products, amylalcohol, and other head roducts such as aldehydes,ethers and the ike. In column '3 no dilu tion takes place, and the tailproducts after being condensed on the shelves of column 3, run down tothe base thereof, and are drawn ofi' through a pipe 9 to a refrigerator10 and to testing ap aratus 11 where the workman ascertains tiiathead'and tail products are passing off, and thence to casks, or vats.The tail products drawn ofi mark 39 to 40 Bau'm. The head products passfrom column.3 into the base of condenser C, and thence through pipe 18to another condenser or refrigerator R, where they are mostlycondensed,'and drawn as by pipe It, controlled by the cock 13. In thetesting apparatus 12 the head products mark' 4243 Baum. Any tailproducts that might be carried along u into condenser C, become therecondense and (fall back onto the shelves of column 3, while the headproducts condensed in R and not extracted through h".pass back-into;condenser C through pipe A 21, whereas the non-condensable gases, forexample, 00,, escapes into the open air through the open pipe 25. Thetemperature in condenser C. is approximately 78 0., but, in order towork at its best, the condenser should be hot atthe top and cold at thebottom. Any usual system of cooling may be used for the condenser, suchas the automatic one illustrated in the drawing.

Having thus fully illustrated and described my invention, what I claimis:

1. The hereindescribed process of purifying alcoholic liquids whichcomprises diluting the same to form a liquid from which head productsand tail products can be simultaneously distilled, directly introducingsaid, liquid into a column still at a point above its base anddistilling it to form vapors containing head products, tail products anda limited amount of ethyl alcohol, treating the vapors with a modicum ofhotaqueous liquid to hold back said ethyl alcohol, collectin dilutepurified alcohol at the base of the st1ll and collecting head productsand tail products near the top of the still.

2. The hereindescribed process of purifying alcoholic liquids whichcomprises diluting the same with-water to form a liquid of between 13.7and 14.7 Baum, introducing the liquid into a column still at a pointabove its base and distilling it to form 5 point above its base anddistilling itto form vapors containing tail products head prodvaporscontaining tail products head prodnets and a limited amount of ethylalcohol, nets and a limited amount of ethyl alcohol, treating the vaporswith a modicum of hot .treating the vapors with a modicum of Water waterto hold back said ethyl alcohol, 001- to hold back said ethyl alcohol,collecting lectiug; dilute purified alcohol at the base of 20 dilutepurified alcohol at'the base of the the still and collecting headproducts and still and collecting head products and tail tail productsnear the top of the still. product svnear the-top of the still. Inwitness whereof I have hereunto set 3. The hereindescribed process ofpurifymy hand in the presence of two witnesses.

' ing alcoholic liquids which comprises dilutl EMILE GUILLAUME.

ing the same wit-h water to form a liquid \Vitnesscs: of between-131 and14.7 Baum, int-ro- Emvgum P. MACLEAN,

du'cing the liquid into a column still ata l I JULES FAYonLET.

